ABSTRACT
Isotope analysis of Sn plays a crucial role in geochemical studies and in monitoring nuclear contamination. Nevertheless, prevalent analytical techniques for examining Sn isotopes encounter the issue of isobaric interference, markedly impacting the accuracy of the test results. Laser resonance ionization mass spectrometry (LRIMS) can effectively overcome the difficulties associated with the isobaric interference inherent in commercial mass spectrometry. In this paper, different amounts of Sn were prepared on Re filaments by electrodeposition and tested via LRIMS. The results showed that the average detection efficiency of LRIMS decreased with increasing total Sn content from 1 µg to 4 µg, and the fluctuations in the test results among the samples increased significantly. Therefore, the electrodeposition process, as well as the composition and morphology of the deposits were characterized by SEM, EDS and XPS; results showed that the degradation of the samples with increasing Sn content was attributed to the complexity of the composition, micro-structure, valence of the deposits, and the interference of various elements. To cope with the anomalies encountered above, the deposits were heat-treated at 600 °C in a hydrogen atmosphere to eliminate detrimental impurities, like Cl, and Sn was effectively reduced to an almost singular atomic state. Furthermore, a titanium layer was covered on the surface of the heat-treated deposit by magnetron sputtering. Ultimately, a highly efficient and stable Sn atomic beam source with a sandwiched structure has been successfully developed and exhibits broad application prospect.
ABSTRACT
The isotopic analysis of Sn is crucial for geochemical research and surveillance of nuclear contamination. However, commonly used methods face the challenge of isobaric interference. Laser resonance ionization mass spectrometry (LRIMS) is a promising technology for effectively eliminating the isobaric interference effect as it combines the advantages of both resonance ionization and mass spectrometry technologies. In this study, an atomic source of 1 µg Sn was prepared by electrodeposition on a Re filament in a 1-5 × 0.7 mm spot for LRIMS measurement. The effects of voltage, duration, length of the active area, and Pb content on the deposition yield were studied, and the morphology, composition, and valence of the Sn deposits were examined. A maximum yield of over 90% in a 3 × 0.7 mm spot was achieved through the surface modification of Re filaments and optimisation of the electrodeposition parameters. As the Sn0 atomic state was predominant in the deposit, the average detection efficiency of the LRIMS device using the as-deposited Sn samples was approximately 3.63 × 10-4, which was almost an order of magnitude higher than that of the sample dropped with graphene oxide solution (4.39 × 10-5).
